関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Piperidine | HCID 8082 | — |
| 反応物 | 4-(3-Chloro-indazole-1-sulfonyl)-N-(4-fluoro-benzyl)-benzamide | HCID 58975152 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(4-Fluoro-benzyl)-4-(3-piperidin-1-yl-indazole-1-sulfonyl)-benzamide | HCID 58975199 | 7% |
反応手順
Dissolve 4-(3-chloro-indazole-1-sulfonyl)-N-(4-fluoro-benzyl)-benzamide (91 mg, 0.20 mmol) in piperidine (11.0 mL) and stir at 90° C. overnight. Dilute the solution with EtOAc (30 mL) and wash with 1N HCl (15 mL) and satd NaHCO3 (15 mL). Dry, filter and concentrate the organic solution and purify the residue by flash chromatography, using a linear gradient of 100% hexanes to 50% EtOAc/hexanes, to give the title compound as a light yellow foam (7 mg, 7%). MS (ES) 493.0 (M+1)+, 491.2 (M−1)−.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07595339B2 |
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| 出典データセット | uspto-grants-2009_09 |
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| ORD ID | ord-4d824759db4846128ba87caf806cc000 |
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| 出典メモ | uspto-grants-2009_09 |
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